工程科学学报，第40卷，第11期：1325-1331,2018年11月 Chinese Joural of Engineering,Vol.40,No.11:1325-1331,November 2018 DOI:10.13374/j.issn2095-9389.2018.11.006;http://journals.ustb.edu.cn 硫化锑精矿还原固硫焙烧直接产出金属锑研究 欧阳臻”，陈艺锋)，胡宇杰)，唐朝波》，陈永明)，叶龙刚) 1)湖南工业大学治金与材料工程学院，株洲4120072)中南大学治金与环境学院，长沙410083 ☒通信作者，E-mail:yelonggang(@sina.cn 摘要针对现行鼓风炉挥发（熔炼）-反射炉还原炼锑工艺存在的流程长、能耗高、低浓度0，烟气污染等问题，提出了一种 基于选治联合过程的锑提取新工艺一硫化锑精矿还原固硫培烧直产金属锑.分别以Z0和碳粉作为固硫剂和还原剂实现 对硫化锑矿的固硫还原转化，直接产出金属锑，同时生成硫化锌，再分别分离得到金属锑粉和硫化锌精矿.本文采用控制变量 法，分别考察了焙烧温度、碳粉粒度，Z0配入量、焙烧时间对锑生成率和Z0固硫率的影响.得到最佳条件如下：焙烧温度 800℃、碳粉粒度100~150目、Z0量为固硫所需理论量、培烧时间2h.在此条件下，锑生成率为90.4%，Z0固硫率为 94.8%,其中温度和Z0加入量对焙烧效果有较大影响：同时对反应产物的分析和过程热力学计算表明焙烧过程分两步进 行，即首先发生Sb,S与Z0的交互固硫反应生成Sb,0,其后在高于700℃温度下Sb20,被大量还原成金属锑.在不同品位 的锑精矿旷综合实验中，均获得了90%左右的锑生成率和88%的固硫率，验证了工艺的可行性.新工艺低温低碳、清洁环保，易 于开展工业化生产 关键词锑治炼：硫化锑：固硫培烧：选治联合：清洁冶金：次氧化锌 分类号TF8 Direct production of antimony by reduction and sulfur-fixing roasting from stibinite concentrate OUYANG Zhen),CHEN Yi-feng,HU Yu-jie,TANG Chao-bo2),CHEN Yong-ming?),YE Long-gang 1)College of Metallurgy and Material Engineering,Hunan University of Technology,Zhuzhou 412007,China 2)School of Metallurgy and Environment,Central South University,Changsha 410083,China Corresponding author,E-mail:yelonggang@sina.cn ABSTRACT Blast furnace volatilizing (smelting)and reverberatory furnace process is the main reduction method in the current anti- mony smelting process,and it is associated with problems such as a long production flow,high energy consumption,and SO flue gas pollution.Thus,in this paper,a new process,based on the combination of beneficiation and metallurgy,was proposed for the direct extraction of antimony from stibnite concentrate.Using ZnO and carbon as a sulfur-fixing agent and reductant,respectively,antimony sulfide was transformed to Sb and ZnS metals,and then the mixture was separated by a mineral separation method.The effects of calci- nation temperature,carbon particle size,ZnO dosage,and calcination time on the conversion rate of Sb and sulfur-fixing rate of ZnO were investigated in detail by controlled variables method.The optimal conditions are as follows:calcination temperature 800 C,car- bon particle size 100~150 mesh,ZnO dosage 1.0 times the theoretical amount,and roasting time 2h.Under these conditions,the an- timony generation rate and sulfur-fixing rate of ZnO are 90.4%and 94.8%,respectively.The antimony generation rate and sulfur-fix- ing rate of Zno can be improved by increasing the reaction temperature and ZnO dosage.Meanwhile,the phase analysis results of the reaction products and thermodynamic calculations of reactions indicate that the reaction paths of SbS,and Zno comprise two steps: First,SbS,reacts with ZnO to generate Sb2O,and then after 700C,it is reduced to a large amount of antimony.In the comprehen- 收稿日期：2017-11-28工程科学学报,第 40 卷,第 11 期:1325鄄鄄1331,2018 年 11 月 Chinese Journal of Engineering, Vol. 40, No. 11: 1325鄄鄄1331, November 2018 DOI: 10. 13374 / j. issn2095鄄鄄9389. 2018. 11. 006; http: / / journals. ustb. edu. cn 硫化锑精矿还原固硫焙烧直接产出金属锑研究 欧阳臻1) , 陈艺锋1) , 胡宇杰1) , 唐朝波2) , 陈永明2) , 叶龙刚1)苣 1) 湖南工业大学冶金与材料工程学院, 株洲 412007 2) 中南大学冶金与环境学院, 长沙 410083 苣 通信作者,E鄄mail: yelonggang@ sina. cn 摘 要 针对现行鼓风炉挥发(熔炼)鄄鄄反射炉还原炼锑工艺存在的流程长、能耗高、低浓度 SO2 烟气污染等问题,提出了一种 基于选冶联合过程的锑提取新工艺———硫化锑精矿还原固硫焙烧直产金属锑. 分别以 ZnO 和碳粉作为固硫剂和还原剂实现 对硫化锑矿的固硫还原转化,直接产出金属锑,同时生成硫化锌,再分别分离得到金属锑粉和硫化锌精矿. 本文采用控制变量 法,分别考察了焙烧温度、碳粉粒度、ZnO 配入量、焙烧时间对锑生成率和 ZnO 固硫率的影响. 得到最佳条件如下:焙烧温度 800 益 、碳粉粒度 100 ~ 150 目、ZnO 量为固硫所需理论量、焙烧时间 2 h,在此条件下,锑生成率为 90郾 4% ,ZnO 固硫率为 94郾 8% ,其中温度和 ZnO 加入量对焙烧效果有较大影响;同时对反应产物的分析和过程热力学计算表明焙烧过程分两步进 行,即首先发生 Sb2 S3 与 ZnO 的交互固硫反应生成 Sb2O3 ,其后在高于 700 益温度下 Sb2O3 被大量还原成金属锑. 在不同品位 的锑精矿综合实验中,均获得了 90% 左右的锑生成率和 88% 的固硫率,验证了工艺的可行性. 新工艺低温低碳、清洁环保,易 于开展工业化生产. 关键词 锑冶炼; 硫化锑; 固硫焙烧; 选冶联合; 清洁冶金; 次氧化锌 分类号 TF8 收稿日期: 2017鄄鄄11鄄鄄28 Direct production of antimony by reduction and sulfur鄄fixing roasting from stibinite concentrate OUYANG Zhen 1) , CHEN Yi鄄feng 1) , HU Yu鄄jie 1) , TANG Chao鄄bo 2) , CHEN Yong鄄ming 2) , YE Long鄄gang 1)苣 1) College of Metallurgy and Material Engineering, Hunan University of Technology, Zhuzhou 412007, China 2) School of Metallurgy and Environment, Central South University, Changsha 410083, China 苣 Corresponding author, E鄄mail: yelonggang@ sina. cn ABSTRACT Blast furnace volatilizing (smelting) and reverberatory furnace process is the main reduction method in the current anti鄄 mony smelting process, and it is associated with problems such as a long production flow, high energy consumption, and SO2 flue gas pollution. Thus, in this paper, a new process, based on the combination of beneficiation and metallurgy, was proposed for the direct extraction of antimony from stibnite concentrate. Using ZnO and carbon as a sulfur鄄fixing agent and reductant, respectively, antimony sulfide was transformed to Sb and ZnS metals, and then the mixture was separated by a mineral separation method. The effects of calci鄄 nation temperature, carbon particle size, ZnO dosage, and calcination time on the conversion rate of Sb and sulfur鄄fixing rate of ZnO were investigated in detail by controlled variables method. The optimal conditions are as follows: calcination temperature 800 益 , car鄄 bon particle size 100 ~ 150 mesh, ZnO dosage 1郾 0 times the theoretical amount, and roasting time 2 h. Under these conditions, the an鄄 timony generation rate and sulfur鄄fixing rate of ZnO are 90郾 4% and 94郾 8% , respectively. The antimony generation rate and sulfur鄄fix鄄 ing rate of ZnO can be improved by increasing the reaction temperature and ZnO dosage. Meanwhile, the phase analysis results of the reaction products and thermodynamic calculations of reactions indicate that the reaction paths of Sb2 S3 and ZnO comprise two steps: First, Sb2 S3 reacts with ZnO to generate Sb2O3 , and then after 700 益 , it is reduced to a large amount of antimony. In the comprehen鄄